CN111217319B - Preparation method of one-dimensional ZnO nano heterojunction array - Google Patents
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Abstract
The invention discloses a preparation method of a one-dimensional ZnO nano heterojunction array, which comprises the following steps: preprocessing a one-dimensional ZnO nanowire array; preparing a precursor solution; preparing a one-dimensional ZnO nano heterojunction array: 1. absorbing a proper amount of precursor solution, dripping the precursor solution into the ZnO nanowire array B, and standing for 10-15 s after the liquid is completely dispersed; 2. placing the other ZnO nanowire array A on the array B in a mode that the back surface of the substrate faces upwards vertically, placing a constant-value weight at the center of the back surface of the substrate of the array A, standing for 5-10 min, and moving the precursor solution from the array B to the array A upwards; 3. and taking down the array A from the array B, keeping the back of the substrate of the array A vertically downward, and then carrying out annealing treatment to obtain the array A, namely the prepared one-dimensional ZnO nano heterojunction array. The method has the advantages of simple operation, low cost and good repeatability, and can be used for large-scale production.
Description
Technical Field
The invention relates to a novel material preparation method, in particular to a preparation method of a one-dimensional ZnO nano heterojunction array.
Background
ZnO is a wide bandgap semiconductor, has a bandgap of about 3.37eV at room temperature, is an important direct bandgap semiconductor, and has very excellent optical characteristics. However, due to the large electron effective mass and the low intrinsic electron mobility, it has been desired to further improve the electrical properties of ZnO by different methods. One-dimensional nanocrystallization and doping of other elements are effective methods for widening the application range of ZnO semiconductor materials and breaking through performance bottlenecks.
The one-dimensional ZnO nano heterojunction array is prepared by doping different impurities by MOCVD (metal chemical vapor deposition), ion implantation, hydrothermal synthesis and other methods on the basis of preparing one-dimensional semiconductor nano materials (nanowires, nanorods and nanotubes) to prepare the nano material with a special demarcation region structure. The unique electrical properties of the material can be obtained by regulating the energy band structure and the electron concentration of the material.
However, the conventional one-dimensional ZnO nano-heterojunction array is generally prepared by a "top-down" technology route, wherein the manufacturing process is completed by starting from a substrate or a thin film, through a high-precision planar lithography technology, and performing processes such as implantation, etching, deposition and the like. Not only the process flow is complex, but also precise and expensive equipment is required to be used, and a plurality of technical difficulties are required to be overcome. Especially for the mainstream integrated circuit at present, the process size and the circuit integration degree are restricted by physical limit and economic cost, and the top-down method puts higher requirements on equipment and a manufacturing process, so that the cost is greatly increased, and the process limitation is more and more obvious.
In summary, the conventional synthesis process of the top-down one-dimensional ZnO nano heterojunction array generally has the limitations of complex operation, high price and low production efficiency. At present, a method which is simple to operate, low in cost and has certain scale and repeatability is not used for preparing the one-dimensional ZnO nano heterojunction array.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the preparation method of the one-dimensional ZnO nano heterojunction array, which is simple to operate, low in cost and good in repeatability.
In order to achieve the above object, the present invention is realized by:
a preparation method of a one-dimensional ZnO nano heterojunction array comprises the following steps:
pretreatment of the one-dimensional ZnO nanowire array: selecting two one-dimensional ZnO nanowire arrays vertically and uniformly grown on a substrate, respectively naming the two one-dimensional ZnO nanowire arrays as an array A and an array B, and then drying the arrays A and B for later use;
preparing a precursor solution: firstly, dissolving indium salt, gallium salt and zinc salt In a solvent according to the atomic ratio of In: ga: zn = 1;
preparing a one-dimensional ZnO nano heterojunction array:
and 3, taking down the array A from the array B, keeping the back of the substrate of the array A vertically downward, and then annealing the array A to obtain the array A, namely the prepared one-dimensional ZnO nano heterojunction array.
Further, the drying of the arrays A and B is realized by drying in a drying oven at 120-150 ℃ for 1-2 h.
Furthermore, two one-dimensional ZnO nanowire arrays which are vertically and uniformly grown on the substrate are selected, the array area is the same macroscopically, the length of the whole nanowire is the same microscopically, the nanowire array and the substrate are of a vertical structure, the angle formed by the nanowire array is 90 degrees +/-10 degrees, and the difference of the arrangement distance of the single nanowire is less than 5 mu m.
Further, dripping the precursor solution into the ZnO nanowire array B according to the amount of the precursor solution and the amount of the precursor solutionArray area 0.5 μ L: 10-20 mm 2 Is carried out in the same manner as described above.
Furthermore, the whole area of the array of the two selected one-dimensional ZnO nanowire arrays is 10-30 mm 2 The whole height of the nanowire is 10-30 mu m; dripping 0.5-1 mu L of precursor solution into the ZnO nanowire array B; 1-5 pieces of 10N constant-value weights are placed in the center of the back face of the substrate of the ZnO nanowire array A, the acting force is changed by changing the number of the constant-value weights, and the degree of wrapping the array A nanowires by the precursor is regulated.
Further, the indium salt is indium nitrate, the gallium salt is gallium nitrate, and the zinc salt is zinc acetate.
Furthermore, the solvent is ethylene glycol monomethyl ether.
Further, the stabilizing agent used is 0.5mol/L ethanolamine.
Further, the step of heating and stirring the mixed solution is to stir the mixed solution in a water bath heating magnetic stirrer in a sealed environment, wherein the water bath temperature is 70-80 ℃, the stirring time is 60-70 min, and the rotating speed is 600-700 rp/m; and the aging is to perform standing aging on the transparent and uniform liquid formed after heating and stirring at room temperature for 36 to 48 hours to obtain the In-Ga-Zn-O transparent precursor solution.
Further, the annealing treatment is that the temperature is kept at 100-150 ℃ for 30-40 min, then the annealing treatment is carried out at 700-900 ℃ for 25-30 min, and then the annealing treatment is carried out in the air to cool the annealing treatment to the room temperature.
The invention has the beneficial effects that:
(1) The invention provides a new method for preparing a one-dimensional ZnO nano heterojunction array.
(2) The method has the advantages of simple operation, low cost and good repeatability, and can be used for large-scale production.
(3) The one-dimensional ZnO nano heterojunction array prepared by the method has good uniformity and stability, and opens up a new idea for the synthesis of a nanowire array device in the future.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a process flow diagram of a one-dimensional ZnO nanowire heterojunction array a prepared in an embodiment of the present invention.
Fig. 2 is a diagram of a one-dimensional ZnO nanowire array a and B selected in embodiment 1 of the present invention.
FIG. 3 is a side view of an optical microscope under an ultraviolet fluorescent lamp of a selected one-dimensional ZnO nanowire array of example 1 of the present invention (a) array A; (B) array B.
Fig. 4 is an optical microscopic side view of the one-dimensional ZnO nanowire heterojunction array a prepared in example 1 of the present invention under ultraviolet fluorescence, (a) a 10N vertical force is applied; (b) applying a vertical force of 30N.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art, are within the scope of the present invention.
According to an embodiment of the invention, a preparation method of a one-dimensional ZnO nano heterojunction array is provided, which comprises the following steps:
pretreatment of the one-dimensional ZnO nanowire array: selecting two one-dimensional ZnO nanowire arrays vertically and uniformly grown on a substrate, respectively naming the two one-dimensional ZnO nanowire arrays as an array A and an array B, and then drying the arrays A and B for later use;
preparing a precursor solution: firstly, dissolving indium salt, gallium salt and zinc salt In a solvent according to the atomic ratio of In: ga: zn = 1;
preparing a one-dimensional ZnO nano heterojunction array:
and 3, taking down the array A from the array B, keeping the back of the substrate of the array A vertically downward, and then annealing the array A to obtain the array A, namely the prepared one-dimensional ZnO nano heterojunction array.
In the pretreatment process of the one-dimensional ZnO nanowire array, the drying of the arrays A and B refers to drying at 120-150 ℃ for 1-2 h by using a drying oven.
The selected two one-dimensional ZnO nanowire arrays which are vertically and uniformly grown on the substrate are required to have the same array area in a macroscopic view, namely the nanowires have the same length in a microscopic view, the nanowires are in a vertical structure with the substrate, the formed angle is 90 degrees +/-10 degrees, and the difference of the arrangement distance of the single nanowires is less than 5 mu m.
In the embodiment of the invention, the precursor solution is dripped into the ZnO nanowire array B according to the proportion that the total area of the precursor solution and the array is 0.5 mu L: 10-20 mm 2 Is carried out in the same manner as described above.
In the embodiment of the invention, the whole area of the two one-dimensional ZnO nanowire arrays is 10-30 mm 2 The whole height of the nanowire is 10-30 mu m; dripping 0.5-1 mu L of precursor solution into the ZnO nanowire array B; 1-5 pieces of 10N constant-value weights are placed in the center of the back face of the substrate of the ZnO nanowire array A, an acting force in the range of 10-50N is applied, the acting force is changed by changing the number of the constant-value weights, and the degree of wrapping the array A nanowires by the precursor is regulated and controlled. In practical operation, the vertical force applied to the back surface of the substrate and the area of the nanowire array (0.6-3) can be 1 (N: mm) 2 ) Is increased or decreased synchronouslyTo place a fixed value weight.
In the embodiment of the invention, the indium salt is indium nitrate, the gallium salt is gallium nitrate, and the zinc salt is zinc acetate. The solvent is ethylene glycol methyl ether. The stabilizer used is 0.5mol/L ethanolamine.
Wherein the step of heating and stirring the mixed solution is to stir the mixed solution in a water bath heating magnetic stirrer in a sealed environment, the water bath temperature is 70-80 ℃, the stirring time is 60-70 min, and the rotating speed is 600-700 rp/m; and the aging is to perform standing aging on the transparent and uniform liquid formed after heating and stirring at room temperature for 36 to 48 hours to obtain the In-Ga-Zn-O transparent precursor solution.
Wherein the annealing treatment is that the temperature is kept at 100-150 ℃ for 30-40 min, then the annealing treatment is carried out at 700-900 ℃ for 25-30 min, and then the annealing treatment is carried out in the air to cool the annealing treatment to the room temperature.
In the embodiment of the invention, the used one-dimensional ZnO nanowire array is prepared by the subject group by a CVD (chemical vapor deposition) method, the prepared ZnO nanowire array has high purity and good collimation degree (vertical to a substrate and the angle is 90 degrees +/-10 degrees), the arrangement distance of single nanowires is less than 5 microns, the whole height is uniform, and the length range is 5-40 microns. The area range of the array prepared at one time is 5-50mm 2 。
The following is a detailed description of specific embodiments.
Example 1
The preparation method of the one-dimensional ZnO nanowire heterojunction array comprises the following specific implementation modes:
(1) Pretreatment of the one-dimensional ZnO nanowire array: firstly, a one-dimensional ZnO nanowire array A (the array area is 10 mm) is selected 2 The overall height of the nanowire is 30 μm, the vertical angle with the substrate is 90 ° ± 10 °, the arrangement distance of the single nanowire is less than 5 μm), and a one-dimensional ZnO nanowire array B (the array area is 10mm2, the overall height of the nanowire is 30 μm, the vertical angle with the substrate is 90 ° ± 10 °, the arrangement distance of the single nanowire is less than 5 μm) are shown in fig. 2, which is a real object diagram of the one-dimensional ZnO nanowire array a and B selected in example 1. Arrays A and B were then placed in a dry box and incubated at 150 ℃ for 1h (see step (1) of FIG. 1).
(2) Preparing a precursor solution: firstly, 5363 g of indium nitrate 0.4210g, 3242 g of gallium nitrate 0.3647g and 4736 g of zinc acetate 0.2743g are weighed and dissolved in 20ml of ethylene glycol monomethyl ether, and then 60. Mu.l of ethanolamine is slowly added thereto by using a single-channel pipette. Further, the mixture was heated in a water bath in a sealed environment at 80 ℃ and magnetically stirred for 70min (rotation speed 700 rp/m) to form a transparent and uniform liquid. Further, standing and aging the precursor at room temperature for 48h to obtain an In-Ga-Zn-O transparent precursor solution.
(3) Preparing a one-dimensional ZnO nano heterojunction array: firstly, the ZnO nanowire array A (selected in the step 1) is slowly vertically turned for 180 degrees and then placed on a cleaned dry glass plate (see the step (2) in the figure 1), then a single-channel pipettor is used for sucking 0.5 mu L of precursor solution (prepared in the step 2) and slowly dropping the precursor solution into the ZnO nanowire array B (selected in the step 1), and the ZnO nanowire array A is placed for 15s (see the step (2) in the figure 1) after the liquid is completely dispersed. Further, the array A is slowly moved above the array B, a 10N constant value weight is placed in the center of the back face of the array A, standing is carried out for 10min, and the precursor solution moves upwards from the array B to wrap the nanowire of the array A. The degree of wrapping the nanowire in the array A by the precursor (10N vertical downward force is added, the precursor wraps 15% of the nanowire in the array A, 30N vertical downward force is added, and the precursor wraps 45% of the nanowire in the array A) can be regulated and controlled by changing the number of the fixed-value weights and further changing the acting force (see step (3) in FIG. 1), and further the doping range is controlled. Further, the array A was removed from the array B, the back surface of the substrate of the array A was kept facing downward vertically, and the substrate was kept at 150 ℃ for 40min, followed by annealing at 900 ℃ for 30min and cooling in air to room temperature. The array A is the prepared one-dimensional ZnO nano heterojunction array. (see step (4) of FIG. 1).
Example 2
The preparation method of the one-dimensional ZnO nanowire heterojunction array comprises the following specific implementation modes:
(1) Pretreatment of the one-dimensional ZnO nanowire array: firstly, a one-dimensional ZnO nanowire array A (the array area is 30 mm) is selected 2 The whole height of the nanowire is 30 mu m, the vertical angle with the substrate is 90 +/-10 degrees, the arrangement distance of a single nanowire is less than 5 mu m, and the one-dimensional ZnO nanowire array B (the array area is 30mm & lt 2 & gt, the whole height of the nanowire is 30 mu m, the vertical angle with the substrate is 90 +/-10 degrees, and the arrangement distance of the single nanowire is less than 5 mu m) is formed. Then the array is putA and B were placed in a drying oven and incubated at 150 ℃ for 1h (see step (1) of FIG. 1).
(2) Preparing a precursor solution: firstly, weighing 2.1050g of indium nitrate, 1.8235g of gallium nitrate and 1.3715g of zinc acetate, dissolving the indium nitrate, the gallium nitrate and the gallium nitrate in 20ml of ethylene glycol monomethyl ether, and then slowly adding 300 mu l of ethanolamine into the ethylene glycol monomethyl ether by using a single-channel pipette. Further, the mixture was heated in a water bath in a sealed environment at 70 ℃ and magnetically stirred for 60min (rotation speed 600 rp/m) to form a transparent and uniform liquid. Further, standing and aging the precursor at room temperature for 36h to obtain the In-Ga-Zn-O transparent precursor solution.
(3) Preparing a one-dimensional ZnO nano heterojunction array: firstly, slowly vertically turning a ZnO nanowire array A (selected in step 1) for 180 degrees, standing on a cleaned dry glass plate (see step (2) in figure 1), then sucking 1 mu L of precursor solution (prepared in step 2) by using a single-channel pipette, slowly dropping the precursor solution into the ZnO nanowire array B (selected in step 1), and standing for 10s (see step (2) in figure 1) after the liquid is completely dispersed. Further, the array A is slowly moved above the array B, two 10N constant value weights are placed at the center of the back face of the array A, then standing is carried out for 5min, and the precursor solution moves upwards from the array B to wrap the nanowire of the array A. By changing the number of the constant-value weights and further changing the acting force, the degree of wrapping the array A nanowire by the precursor (20N vertical downward acting force is added, the precursor wraps 15% of the array A nanowire as a whole, 50N vertical downward acting force is added, and the precursor wraps 45% of the array A nanowire as a whole) can be regulated and controlled (see step (3) in fig. 1), and the doping range is further controlled. Further, the array A was removed from the array B, the substrate of the array A was kept with its back surface facing vertically downward, and the temperature was maintained at 100 ℃ for 30min, followed by annealing at 700 ℃ for 25min and cooling in air to room temperature. The array A is the prepared one-dimensional ZnO nano heterojunction array. (see step (4) of FIG. 1).
FIG. 3 is the optical microscopic side view of the one-dimensional ZnO nanowire array selected in example 1 under an ultraviolet fluorescent lamp (a) array A; (B) array B. The ZnO nanowire has the property of exciting green fluorescence under the irradiation of ultraviolet light, so that the one-dimensional ZnO nanowire array with the selected array A, B as components and uniform length can be proved.
Fig. 4 is an optical microscopic side view of the one-dimensional ZnO nanowire heterojunction array a prepared in example 1 under ultraviolet fluorescence, (a) a 10N vertical force is applied; (b) applying a vertical force of 30N. As can be seen from fig. 4, the upper half of the nanowire array a emits yellow light, which is due to the fact that the upper end portion is doped with In and Ga elements, the energy band structure and the electron transport property of the nanowire are changed, yellow fluorescence is excited by ultraviolet light, and synthesis of the one-dimensional ZnO nano heterojunction array is achieved. The yellow fraction accounted for 15% and 45% of the total with different applied forces of 10N and 30N, demonstrating that the doping range can be varied by varying the applied vertical force.
The invention abandons the traditional fussy and expensive 'top-down' nanowire array preparation method, prepares the one-dimensional ZnO nano heterojunction array by a simple and cheap method, and opens up a new idea for the construction of one-dimensional ZnO nano heterojunction array devices such as light-emitting diodes, ultraviolet detectors, field effect transistors and the like.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention.
Claims (2)
1. A preparation method of a one-dimensional ZnO nano heterojunction array is characterized by comprising the following steps:
pretreatment of the one-dimensional ZnO nanowire array: selecting two one-dimensional ZnO nanowire arrays vertically and uniformly grown on a substrate, respectively naming the two one-dimensional ZnO nanowire arrays as an array A and an array B, and then drying the arrays A and B for later use;
preparing a precursor solution: firstly, dissolving indium salt, gallium salt and zinc salt In a solvent according to the atomic ratio of In: ga: zn = 1;
preparing a one-dimensional ZnO nano heterojunction array:
step 1, sucking a proper amount of prepared precursor solution, slowly dripping the precursor solution into a ZnO nanowire array B, and standing for 10-15 s after the liquid is completely dispersed;
step 2, placing the other ZnO nanowire array A on the ZnO nanowire array B in a mode that the back surface of the substrate faces upwards vertically, placing a constant-value weight at the center of the back surface of the substrate of the ZnO nanowire array A according to the acting force of 10-50N, standing for 5-10 min, and moving the precursor solution from the array B to the array A upwards;
step 3, taking down the array A from the array B, keeping the back of the substrate of the array A vertically downward, and then annealing the array A to obtain an array A, namely the prepared one-dimensional ZnO nano heterojunction array;
two one-dimensional ZnO nanowire arrays which are vertically and uniformly grown on a substrate are selected, the one-dimensional ZnO nanowire arrays have the same array area in a macroscopic view, the nanowires have the same overall length in a microscopic view, a vertical structure is formed between the nanowires and the substrate, the formed angle is 90 degrees +/-10 degrees, and the difference of the arrangement space of the single nanowire is less than 5 mu m;
and (3) dropwise adding the precursor solution into the ZnO nanowire array B according to the ratio of the precursor solution to the whole area of the array of 0.5 mu L: 10-20 mm 2 The ratio of (a) to (b);
the whole area of the array of the two selected one-dimensional ZnO nanowire arrays is 10-30 mm 2 The whole height of the nanowire is 10-30 mu m; dripping 0.5-1 mu L of precursor solution into the ZnO nanowire array B; 1-5 pieces of 10N constant value weights are placed in the center of the back face of the substrate of the ZnO nanowire array A, the acting force is changed by changing the number of the constant value weights, and the degree of wrapping the array A nanowires by a precursor is regulated and controlled;
the indium salt is indium nitrate, the gallium salt is gallium nitrate, and the zinc salt is zinc acetate;
the solvent is ethylene glycol monomethyl ether;
the stabilizing agent is 0.5mol/L ethanolamine;
the step of heating and stirring the mixed solution is to stir the mixed solution in a water bath heating magnetic stirrer in a sealed environment, wherein the water bath temperature is 70-80 ℃, the stirring time is 60-70 min, and the rotating speed is 600-700 rp/m; aging, namely standing and aging the transparent and uniform liquid formed after heating and stirring at room temperature for 36-48 h to obtain an In-Ga-Zn-O transparent precursor solution;
the annealing treatment is that the temperature is kept at 100-150 ℃ for 30-40 min, then the annealing treatment is carried out at 700-900 ℃ for 25-30 min, and then the annealing treatment is carried out in the air to cool the annealing treatment to the room temperature.
2. The method for preparing a one-dimensional ZnO nano heterojunction array according to claim 1, wherein the drying of the arrays A and B is performed by drying in a drying oven at 120-150 ℃ for 1-2 h.
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